CN115612330A - Preparation and application of sulfydryl modified nano silver particle dispersion liquid - Google Patents
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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Abstract
The invention discloses a preparation method and application of a sulfydryl modified nano-silver particle dispersion liquid, wherein a compound with sulfydryl and nano-silver particles with positive charges on the surface are added into ethanol, nitrogen is introduced to remove oxygen, and then the mixture reacts for 1 to 5 hours under the ultrasonic action to obtain a nano-silver particle dispersion liquid with sulfydryl on the surface; wherein the mass fraction of the nano silver particles is 0.1-1%, and the mass ratio of the mercapto compound to the nano silver particles is 0.1-1; the sulfhydryl compound is one or more of cysteine, mercaptoethylamine, 3-sulfhydryl-1-propylamine and 4-amino-2-mercaptopyrimidine. According to the invention, the paint with the surface antibacterial property synergistically enhanced by the graphene/nano-silver particles is prepared by adopting the sulfydryl modified nano-silver particle dispersion liquid, and the problems of low utilization rate of silver components, insufficient antibacterial efficiency and antibacterial durability, poor dispersibility and the like of the existing silver antibacterial paint are solved.
Description
Technical Field
The invention relates to the technical field of chemical coatings, in particular to preparation and application of a sulfydryl modified nano silver particle dispersion liquid.
Background
As the size of the silver particles becomes smaller, the number of atoms on the surfaces of the particles is obviously increased and even is more than that of atoms in the particles, so that a series of excellent performances different from bulk silver are shown, the silver antibacterial coating is widely applied to the aspects of conductive paste, sterilization, catalysis and the like, and the silver antibacterial coating is one of products.
Graphene oxide is a graphene derivative, is a two-dimensional sheet material consisting of a single layer of sp2 hybridized carbon/oxygen atoms, and has peculiar mechanical, electrical, optical, thermal, dispersion, corrosion prevention and other properties due to the special structure, and has physical segmentation and electronic effects on bacteria due to the electronic effect of C = O double bonds and high radius-thickness ratio, so that the graphene oxide has excellent antibacterial and bactericidal effects.
The Chinese patent application CN105419530A, the graphene/nano silver antibacterial coating and the preparation method thereof are characterized in that graphene/nano silver particles are introduced into an aqueous coating to prepare the graphene/nano silver antibacterial coating, but the graphene, the nano silver particles and the aqueous emulsion have poor binding force, so that the nano silver particles and the graphene are not uniformly dispersed, the antibacterial effect cannot be further increased by the cooperation of the introduction of the graphene, and silver ions are difficult to fix in the coating layer, so that the long-acting antibacterial function is difficult to realize.
In the Chinese patent application CN107815193A, the nano silver loaded graphene antibacterial agent and the nano silver loaded graphene in-situ reduction waterborne antibacterial coating, nano silver particles are loaded on a graphene sheet layer and then introduced into the coating.
Chinese patent CN113004732A, an antibacterial coating formulation and a preparation method thereof, form a closed hollow island structure inside a graphene-acrylic acid composite emulsion by composite crosslinking of graphene and acrylic acid, and then add nano silver particles into the coating, which also cannot solve the problem of interface combination and dispersion among resin, nano silver particles and graphene.
Disclosure of Invention
The invention aims to provide preparation and application of a sulfydryl modified nano-silver particle dispersion liquid, and the prepared graphene/nano-silver particle synergistically enhanced surface antibacterial coating solves the problems of low utilization rate of silver components, insufficient antibacterial efficiency and antibacterial durability, poor dispersibility and the like of the existing silver antibacterial coating.
In order to realize the purpose, the invention provides a preparation method and application of a sulfydryl modified nano silver particle dispersion liquid, wherein a compound with sulfydryl and nano silver particles with positive charges on the surface are added into ethanol, nitrogen is introduced to remove oxygen, and then the mixture reacts for 1 to 5 hours under the ultrasonic action to obtain the nano silver particle dispersion liquid with sulfhydrylated surface;
wherein the mass fraction of the nano silver particles is 0.1-1%, and the mass ratio of the mercapto compound to the nano silver particles is 0.1-1;
the sulfhydryl compound is one or more of cysteine, mercaptoethylamine, 3-sulfhydryl-1-propylamine and 4-amino-2-mercaptopyrimidine.
Preferably, the preparation of the nano silver particles comprises the steps of adding 0.1-5% of hydroxyl acrylic monomer, 0.01-0.3% of cationic surfactant and 0.1-3% of silver nitrate into water by mass fraction, and then treating for 1-20 hours under the condition of ultrasonic wave with the power of 100-3000W to obtain the nano silver particles with positive charges on the surface and the size of 5-30 nm.
An application of a sulfydryl modified nano silver particle dispersion liquid in long-acting antibacterial anticorrosive water-based paint.
Preferably, the composition comprises the following components in percentage by mass: 0.5-4% of sulfhydrylation nano silver particle dispersion liquid, 0.05-1% of graphene oxide, 0.05-1% of dispersing agent, 0.1-1% of flatting agent, 1-3% of cross-linking agent, 0.1-2% of thickening agent, 0.1-1% of defoaming agent, 10-40% of water-based acrylic resin and the balance of water.
Preferably, the number of layers of the graphene oxide is 1-10, the sheet diameter is 0.1-3 μm, and the C/O is less than 1.5.
Preferably, the dispersing agent is a low molecular weight polyelectrolyte, and the low molecular weight polyelectrolyte is one or more of polyacrylic acid, hydrolyzed polymaleic anhydride, polyacrylamide, guar gum and arabic resin.
Preferably, the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane and fluorine modified acrylic vinegar.
Preferably, the defoaming agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane and fluorine modified acrylic acid vinegar.
Preferably, the cross-linking agent is one or more of aziridine cross-linking agent, blocked isocyanate curing agent and etherified amino resin; the thickener is at least one of associated alkali swelling thickener and polyurethane thickener.
A preparation method of a long-acting antibacterial anticorrosive water-based paint comprises the steps of adding a certain amount of sulfhydrylation nano silver particle dispersion liquid, graphene oxide, a dispersing agent, a flatting agent, a thickening agent and a defoaming agent into a certain amount of water-based acrylic resin and derivatives thereof, and stirring for 0.5-2 hours at 25-40 ℃ to obtain a finished product.
The invention has the beneficial effects that:
(1)NH 2 amino on the modified silver nanoparticles can react with carboxyl on graphene oxide so as to be fixed on the surface of the graphene oxide, and can also react with carboxyl in resin so as to solve covalent bonding between the resin and the silver nanoparticles, and hydroxyl on the graphene oxide can also react with the carboxyl in the resin so as to solve interface bonding between the graphene and the resin, and a cross-linked network is formed among the silver nanoparticles, the graphene oxide and the resin.
(2) Silver mercaptide nanoparticles: covalent bonds can be formed with Ag through sulfydryl; meanwhile, the positively charged protonated amino groups further improve the stability of the silver nanoparticles.
(3) This application has adopted the ultrasonic wave method to cooperate hydroxyl acrylic acid monomer to realize that the silver ion reduces fast and prepares 5-30nm nanometer silver granule, and the efficiency of reduction is high, and the granularity of product is even, and with direct ultrasonic wave comparison, reduction efficiency is higher and the granularity is more even.
(4) By introducing a small amount of cationic surfactant, silver nanoparticles are formed on the surface of the silver halide colloidal core in the reduction process, positive charge of the silver nanoparticles is realized, and the dispersibility and stability of the silver nanoparticles are ensured.
(5) The coating after crosslinking not only has excellent antibacterial performance, but also can enhance the mechanical property and the compactness of the coating by introducing the graphite oxide, and has higher corrosion resistance.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
Fig. 1 is a structural schematic diagram of a graphene/nano-silver water-based paint of the invention.
Detailed Description
The present invention will be further described with reference to examples, in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
Preparation of Nano silver particles
Adding 3 mass percent of hydroxyl acrylic monomer, 0.1 mass percent of cationic surfactant and 2 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with the power of 1500W to obtain nano silver particles with positive charges on the surface and the particle size of 5-30 nm.
Preparation of sulfhydrylation nano silver particle dispersion liquid
Adding 0.05% of cysteine and 0.5% of nano silver particles with positive charges on the surface into ethanol, introducing nitrogen to remove oxygen, and reacting for 5h under the action of ultrasound to obtain the nano silver particle dispersion liquid with sulfhydrylation on the surface.
Preparation of Water-based paint
Adding 0.5% of sulfhydrylation nano silver particle dispersion liquid, 0.5% of graphene oxide, 0.05% of dispersing agent, 0.1% of flatting agent, 3% of cross-linking agent, 0.1% of thickening agent and 0.1% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 40 ℃ to obtain a finished product.
Example 2
Preparation of Nano silver particles
Adding 3 mass percent of hydroxyl acrylic monomer, 0.1 mass percent of cationic surfactant and 2 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with the power of 1500W to obtain nano silver particles with positive charges on the surface and the particle size of 5-30 nm.
Preparation of sulfhydrylation nano silver particle dispersion liquid
Adding 0.05 percent by mass of 3-mercapto-1-propylamine and 0.5 percent by mass of nano silver particles with positive charges on the surface into ethanol, introducing nitrogen to remove oxygen, and reacting for 5 hours under the action of ultrasound to obtain the nano silver particle dispersion liquid with thiolated surface.
Preparation of Water-based paint
Adding 2% of sulfhydrylation nano silver particle dispersion liquid, 0.5% of dispersing agent, 0.5% of flatting agent, 3% of cross-linking agent, 1% of thickening agent and 0.5% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
Example 3
Preparation of Nano silver particles
Adding 3 mass percent of hydroxyl acrylic monomer, 0.1 mass percent of cationic surfactant and 2 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with the power of 1500W to obtain nano silver particles with positive charges on the surface and the particle size of 5-30 nm.
Preparation of sulfhydrylation nano silver particle dispersion liquid
Adding 0.05% of 4-amino-2-mercaptopyrimidine and 0.5% of nano silver particles with positive surface charges into ethanol, introducing nitrogen to remove oxygen, and reacting for 5 hours under the action of ultrasound to obtain the nano silver particle dispersion liquid with thiolated surface.
Preparation of Water-based paint
Adding 4% of sulfhydrylation nano silver particle dispersion liquid, 1% of graphene oxide, 1% of dispersing agent, 1% of flatting agent, 3% of cross-linking agent, 2% of thickening agent and 1% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
Example 4
Preparation of Nano silver particles
Adding 5 mass percent of hydroxyl acrylic monomer, 0.05 mass percent of cationic surfactant and 3 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with the power of 1500W to obtain nano silver particles with positive charges on the surface and the particle size of 5-30 nm.
Preparation of sulfhydrylation nano silver particle dispersion liquid
Adding 0.05% of 4-amino-2-mercaptopyrimidine and 0.5% of nano silver particles with positive surface charges into ethanol, introducing nitrogen to remove oxygen, and reacting for 5 hours under the action of ultrasound to obtain the nano silver particle dispersion liquid with thiolated surface.
Preparation of Water-based paint
Adding 4% of sulfhydrylation nano silver particle dispersion liquid, 1% of graphene oxide, 1% of dispersing agent, 1% of flatting agent, 3% of cross-linking agent, 2% of thickening agent and 1% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
Example 5
Preparation of Nano silver particles
Adding 4 mass percent of hydroxyl acrylic monomer, 0.2 mass percent of cationic surfactant and 2 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with power of 1500W to obtain nano silver particles with positive charges on the surface and the size of 5-30 nm.
Preparation of sulfhydrylation nano silver particle dispersion liquid
Adding 0.1 mass percent of 4-amino-2-mercaptopyrimidine and 0.5 mass percent of nano silver particles with positive charges on the surface into ethanol, introducing nitrogen to remove oxygen, and reacting for 5 hours under the ultrasonic action to obtain the nano silver particle dispersion liquid with thiolated surface.
Preparation of aqueous coatings
Adding 3% of sulfhydrylation nano silver particle dispersion liquid, 1% of graphene oxide, 1% of dispersing agent, 1% of flatting agent, 2% of cross-linking agent, 1% of thickening agent and 0.2% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
Comparative example 1
Preparation of Nano silver particles
Adding 5 mass percent of hydroxyl acrylic monomer, 0.05 mass percent of cationic surfactant and 3 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with power of 1500W to obtain nano silver particles with positive charges on the surface and the size of 5-30 nm.
Preparation of Water-based paint
Adding 4% of unmodified nano silver particle dispersion liquid, 1% of graphene oxide, 1% of dispersing agent, 1% of flatting agent, 3% of cross-linking agent, 2% of thickening agent and 1% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
Comparative example 2
Preparation of Nano silver particles
Adding 5 mass percent of hydroxyl acrylic monomer, 0.05 mass percent of cationic surfactant and 3 mass percent of silver nitrate into water, and then treating for 16 hours under the condition of ultrasonic wave with the power of 1500W to obtain nano silver particles with positive charges on the surface and the particle size of 5-30 nm.
Preparation of aqueous coatings
Adding 4% of unmodified nano silver particle dispersion liquid, 1% of graphene oxide, 1% of dispersing agent, 1% of flatting agent, 3% of cross-linking agent, 2% of thickening agent and 1% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
Comparative example 3
Preparation of Water-based paint
Adding 1% of dispersing agent, 1% of flatting agent, 3% of cross-linking agent, 2% of thickening agent and 1% of defoaming agent into water-based acrylic resin, and stirring for 2h at 30 ℃ to obtain a finished product.
Comparative example 4
Preparation of Water-based paint
Adding 1% of dispersing agent, 1% of flatting agent, 3% of cross-linking agent, 2% of thickening agent and 1% of defoaming agent into water-based acrylic resin, and stirring for 2 hours at 30 ℃ to obtain a finished product.
The water-based paints prepared in examples 1 to 5 and comparative examples 1 to 4 were subjected to antibacterial property and salt spray property tests.
The water paint prepared in the examples 1-3 and the comparative examples 1 and 3 is pre-coated with an anti-corrosion base coat manually on degreased aluminum foil, and then the anti-bacterial anti-corrosion surface coat is obtained by a manual scraper (baking condition is 260 ℃ multiplied by 20s, then the water is soaked for 300h, after being dried, the antibacterial performance is tested according to GB21551.2-2010 appendix A, and the neutral salt spray test is tested according to JISZ 2371. The results are shown in Table I.
The water paint prepared in the examples 4-5, the comparative examples 2 and the comparative examples 4 is pre-coated with the anti-corrosion base coat manually on a 120X 50X 0.5mm standard steel plate, then the anti-bacterial and anti-corrosion surface coat is manually scraped (the baking condition is 150 ℃ X10 min, then the ultraviolet light aging test is carried out according to GB/T16422.3-2014, the anti-bacterial performance is tested according to GB21551.2-2010 appendix A, the salt spray performance is tested according to JIS Z2371, and the results are shown in the table I.
TABLE-Water-based paint antibacterial and salt spray Performance test data
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of sulfydryl modified nano silver particle dispersion liquid is characterized by comprising the following steps: adding a compound with sulfydryl and nano silver particles with positive charges on the surface into ethanol, introducing nitrogen to remove oxygen, and reacting for 1-5h under the ultrasonic action to obtain nano silver particle dispersion liquid with sulfydryl on the surface;
wherein the mass fraction of the nano silver particles is 0.1-1%, and the mass ratio of the mercapto compound to the nano silver particles is 0.1-1;
the sulfhydryl compound is one or more of cysteine, mercaptoethylamine, 3-sulfhydryl-1-propylamine and 4-amino-2-mercaptopyrimidine.
2. The method for preparing the thiol-modified nano silver particle dispersion liquid according to claim 1, wherein: the preparation of the nano silver particles comprises the steps of adding 0.1-5% of hydroxyl acrylic monomer, 0.01-0.3% of cationic surfactant and 0.1-3% of silver nitrate into water by mass percent, and then treating for 1-20h under the ultrasonic condition with the power of 100-3000W to obtain the nano silver particles with positive charges on the surface and the particle size of 5-30 nm.
3. Use of a dispersion of thiol-modified nano-silver particles according to any one of claims 1-2, characterized in that: is applied to long-acting antibacterial anticorrosive water-based paint.
4. The long-acting antibacterial anticorrosive water-based paint as claimed in claim 3, which is characterized by comprising the following components in percentage by mass: 0.5-4% of sulfhydrylation nano silver particle dispersion liquid, 0.05-1% of graphene oxide, 0.05-1% of dispersing agent, 0.1-1% of flatting agent, 1-3% of cross-linking agent, 0.1-2% of thickening agent, 0.1-1% of defoaming agent, 10-40% of water-based acrylic resin and the balance of water.
5. The long-acting antibacterial anticorrosive water-based paint according to claim 4, characterized in that: the number of layers of the graphene oxide is 1-10, the sheet diameter is 0.1-3 mu m, and the C/O is less than 1.5.
6. The long-acting antibacterial anticorrosive water-based paint according to claim 4, characterized in that: the dispersing agent is low molecular weight polyelectrolyte, and the low molecular weight polyelectrolyte is one or more of polyacrylic acid, hydrolyzed polymaleic anhydride, polyacrylamide, guergain and Arabic resin.
7. The long-acting antibacterial anticorrosive water-based paint according to claim 4, characterized in that: the leveling agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane and fluorine modified acrylic vinegar.
8. The long-acting antibacterial anticorrosive water-based paint according to claim 4, characterized in that: the defoaming agent is one or more of polydimethylsiloxane, alkyl modified organic siloxane and fluorine modified acrylic acid vinegar.
9. The long-acting antibacterial anticorrosive water-based paint according to claim 4, characterized in that: the cross-linking agent is one or more of aziridine cross-linking agent, blocked isocyanate curing agent and etherified amino resin; the thickener is at least one of associated alkali swelling thickener and polyurethane thickener.
10. A method for preparing a long-acting antibacterial anticorrosive water-based paint as claimed in any one of claims 4 to 9, characterized in that: adding a certain amount of sulfhydrylation nano silver particle dispersion liquid, graphene oxide, a dispersing agent, a flatting agent, a thickening agent and a defoaming agent into a certain amount of water-based acrylic resin and derivatives thereof, and stirring for 0.5-2h at 25-40 ℃ to obtain a finished product.
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